WO2023120318A1 - Solution de dépôt autocatalytique et procédé de fabrication de substrat de câblage - Google Patents

Solution de dépôt autocatalytique et procédé de fabrication de substrat de câblage Download PDF

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Publication number
WO2023120318A1
WO2023120318A1 PCT/JP2022/046027 JP2022046027W WO2023120318A1 WO 2023120318 A1 WO2023120318 A1 WO 2023120318A1 JP 2022046027 W JP2022046027 W JP 2022046027W WO 2023120318 A1 WO2023120318 A1 WO 2023120318A1
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WO
WIPO (PCT)
Prior art keywords
electroless plating
ruthenium
plating solution
manufacturing
substrate
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PCT/JP2022/046027
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English (en)
Japanese (ja)
Inventor
正三 新宮原
亮太 齊田
Original Assignee
東京エレクトロン株式会社
学校法人 関西大学
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Application filed by 東京エレクトロン株式会社, 学校法人 関西大学 filed Critical 東京エレクトロン株式会社
Priority to JP2023569342A priority Critical patent/JPWO2023120318A1/ja
Publication of WO2023120318A1 publication Critical patent/WO2023120318A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
    • H05K3/42—Plated through-holes or plated via connections

Definitions

  • the present disclosure relates to an electroless plating solution and a method for manufacturing a wiring board.
  • Patent Document 1 discloses a method of depositing copper in wiring grooves and wiring holes of a substrate by electroless copper plating.
  • Ruthenium (Ru) is attracting attention as a wiring material with the progress of miniaturization of semiconductor wiring in recent years.
  • the ruthenium film can be formed using CVD (Chemical Vapor Deposition), but it is also possible to form the ruthenium film by electroless plating.
  • electroless plating is excellent in productivity and capable of forming metal films of various shapes, and is suitable for manufacturing microstructures such as wiring of semiconductor substrates.
  • the present disclosure provides an advantageous technique for stably depositing ruthenium on a material by electroless plating.
  • One aspect of the present disclosure contains a ruthenium salt, a complexing agent, a reducing agent, and a pH adjusting agent, wherein the reducing agent comprises hydrazine-hydrate, and the complexing agent comprises tartaric acid and ammonium chloride. It relates to an electrolytic plating solution.
  • FIG. 1A is an enlarged cross-sectional view of a substrate showing an example of a first method for manufacturing a wiring substrate.
  • FIG. 1B is an enlarged cross-sectional view of a substrate showing an example of a first method for manufacturing a wiring substrate.
  • FIG. 1C is an enlarged cross-sectional view of the substrate showing an example of the first manufacturing method of the wiring substrate.
  • FIG. 2A is an enlarged cross-sectional view of a substrate showing an example of a second method of manufacturing a wiring substrate.
  • FIG. 2B is an enlarged cross-sectional view of the substrate showing an example of the second manufacturing method of the wiring substrate.
  • FIG. 2C is an enlarged cross-sectional view of the substrate showing an example of the second manufacturing method of the wiring substrate.
  • FIG. 3 is an enlarged cross-sectional view of a substrate showing an example of a third method of manufacturing a wiring substrate.
  • ruthenium is embedded as wiring in recesses (for example, wiring grooves such as trenches and wiring holes such as vias) of a semiconductor substrate (wafer) by electroless plating.
  • the plating solution used in the electroless plating of this embodiment is an electroless plating solution containing a ruthenium salt (that is, an electroless ruthenium plating solution).
  • a ruthenium salt that is, an electroless ruthenium plating solution.
  • the form of the ruthenium salt in the electroless ruthenium plating solution is not limited; state.
  • ruthenium in general including ruthenium ions and ruthenium hydrates contained in the electroless plating solution may simply be referred to as ruthenium salts.
  • the electroless plating solution used in this embodiment further contains a complexing agent, a reducing agent, and a pH adjuster in addition to the ruthenium salt.
  • Reducing agents include hydrazine-hydrate.
  • Complexing agents include tartaric acid and ammonium chloride.
  • electroless plating using the above electroless plating solution is advantageous for stably depositing ruthenium as a plating metal on a material. I got it.
  • the present inventor changed the molar concentration of ruthenium salt (ruthenium chloride (III)-n hydrate: RuCl 3 ⁇ n(H 2 O)), tartaric acid, and ammonium chloride in the electroless plating solution to obtain ruthenium. It was deposited on a substrate as a plated body, and the deposition rate and surface electrical resistivity of the ruthenium were evaluated.
  • ruthenium salt ruthenium chloride (III)-n hydrate: RuCl 3 ⁇ n(H 2 O)
  • Table 1 above shows the evaluation conditions and evaluation results of ruthenium actually deposited on the substrate (that is, sample 1 and sample 2).
  • Table 2 above shows the evaluation conditions common to Sample 1 and Sample 2 shown in Table 1.
  • Ru deposition rate indicates the deposition rate of ruthenium on the substrate, and is expressed by the amount of increase in the thickness direction length of ruthenium per minute (nanometers).
  • Ru surface electrical resistivity indicates the surface electrical resistivity of ruthenium measured immediately after the ruthenium film was formed on the substrate.
  • Ru surface electrical resistivity after forming gas heat treatment indicates the surface electrical resistivity of ruthenium measured after the ruthenium deposited on the substrate is heat treated (annealed) with forming gas. In the heat treatment, a mixed gas of nitrogen and hydrogen was used as a forming gas, and the ruthenium deposited on the substrate was heated using the forming gas at 400° C. for 30 minutes.
  • pH in Table 2 indicates the pH of the electroless plating solution actually used.
  • Bath temperature indicates the temperature of the electroless plating solution actually used (especially the measured temperature of the electroless plating solution on the substrate).
  • the inventor of the present invention has found that the solution containing a complexing agent (tartaric acid and ammonium chloride), a reducing agent (hydrazine-hydrate) and a pH adjusting agent (potassium hydroxide) should be left for two days or more after adding the ruthenium salt.
  • a complexing agent tartaric acid and ammonium chloride
  • a reducing agent hydroazine-hydrate
  • a pH adjusting agent potassium hydroxide
  • a plurality of samples were prepared by changing the molar concentration of tartaric acid (L(+)-tartaric acid) in the electroless plating solution within the range of 10 mol/m 3 to 60 mol/m 3 .
  • a plurality of samples were prepared by changing the molar concentration of ammonium chloride in the electroless plating solution within the range of 10 mol/m 3 to 480 mol/m 3 .
  • a plurality of samples were also prepared in which the molar concentration of ruthenium (III) chloride-n hydrate in the electroless plating solution was 10 mol/m 3 .
  • samples were also prepared using TMAH (tetramethylammonium hydroxide) or sodium hydroxide instead of potassium hydroxide as a pH adjuster.
  • samples 1 and 2 shown in Table 1 the deposition rate of ruthenium was relatively high.
  • the surface electrical resistivity of ruthenium on the substrate after the forming gas heat treatment was relatively low, and had sufficient resistance performance as a wiring embedded in the recess of the semiconductor substrate.
  • the present inventor performed heat treatment (annealing) of ruthenium (plated body) by changing the heating temperature in the range of 0 ° C. to 600 ° C. with respect to a plurality of samples made under the same conditions. treatment) was performed and the surface electrical resistivity was measured. Specifically, for a plurality of samples, heat treatment of ruthenium was performed in a vacuum with an atmospheric pressure of 1 ⁇ 10 ⁇ 3 (Pa) without using a forming gas. For other samples, the ruthenium was heat treated using forming gas.
  • samples using an electroless plating solution containing ruthenium salts, complexing agents (tartaric acid and ammonium chloride), reducing agents (hydrazine-hydrate), and pH adjusters showed ruthenium deposition rate and surface electrical resistivity. was within acceptable limits.
  • the solubility of ammonium chloride, the deposition rate of ruthenium, and the deposition rate and surface electrical resistivity of ruthenium were evaluated for samples with a hydrazine-hydrate (reducing agent) molar concentration of 5 mol/m 3 to 40 mol/m 3 . was good from a comprehensive point of view.
  • samples with a tartaric acid molar concentration of 10 to 100 mol/m 3 and an ammonium chloride molar concentration of 10 to 1000 mol/m 3 gave good evaluation results for the ruthenium deposition rate and the surface electrical resistivity.
  • the electroless plating solution after adjustment with the pH adjuster was alkaline, particularly when it had a pH of 11 or higher (e.g., a pH of 13 or lower), ruthenium could be deposited on the substrate particularly stably.
  • the inventor added ruthenium salt to pure water, but the ruthenium salt did not dissolve in pure water. Also, the inventors added a ruthenium salt to a solution containing only ammonium chloride, but the ruthenium salt did not dissolve in the solution.
  • the inventor performed electroless plating using an electroless ruthenium plating solution containing only ammonium chloride as a complexing agent, but no ruthenium was deposited on the substrate.
  • the inventors performed electroless plating using an electroless ruthenium plating solution containing only tartaric acid as a complexing agent, but no ruthenium was deposited on the substrate.
  • the inventor further evaluated the deposition rate of ruthenium by changing the substrate (material) on which ruthenium was deposited.
  • Table 3 above shows the evaluation conditions common to Samples 3 to 5 shown in Table 4.
  • Table 4 above shows the evaluation results of the deposition rate of Samples 3-5.
  • Table 5 shows the evaluation conditions for Sample 6 shown in Table 6.
  • Table 6 shows the evaluation results of the deposition rate of Sample 6.
  • the inventor further evaluated the elemental ratio (at%) of ruthenium and oxygen in the plated body by changing the content composition ratio of the electroless ruthenium plating solution.
  • Table 7 above shows the evaluation conditions for Samples 7-9.
  • Table 8 above shows the evaluation results of the elemental ratio (at %) of ruthenium and oxygen in the plated body for samples 7-9.
  • Table 8 The row marked with "As depo.” in Table 8 shows the evaluation results for ruthenium immediately after film formation on the substrate.
  • the row labeled “after forming gas heat treatment” in Table 8 shows the evaluation results after the ruthenium deposited on the substrate was heat treated (400° C. for 30 minutes) with forming gas.
  • 1A to 1C are enlarged cross-sectional views of a substrate 10 showing an example of a first method of manufacturing a wiring board.
  • a substrate 10 having recesses 11 for wiring is prepared. Although only one recess 11 is shown in FIGS. 1A-1C, substrate 10 may have multiple recesses 11 .
  • the specific shape and size of the recess 11 are not limited, and typically at least one of trenches (wiring grooves) and vias (wiring holes) can be included in the concept of the recess 11 .
  • the recess partition surface 12 that partitions the recess 11 includes a partition bottom surface 12a and a partition side surface 12b.
  • the compartment bottom surface 12a in this example comprises a metal surface that serves as a substrate on which ruthenium is deposited by electroless plating.
  • the lower layer wiring 22 containing ruthenium forms the division bottom surface 12a, but the lower layer wiring 22 may contain a material other than ruthenium.
  • the partition side surface 12b of this example is formed by the barrier film 21 covering the insulating film 20.
  • the barrier film 21 is a film for preventing the ruthenium embedded in the recess 11 from diffusing into the insulating film 20, and can be made of any metal (for example, Ta (tantalum) or TaN (tantalum nitride)).
  • the electroless plating solution 50 is applied onto the substrate 10 to form a puddle of the electroless plating solution 50, and the recesses 11 are entirely filled with the electroless plating solution 50 as shown in FIG. 1B. This ensures that the electroless plating solution 50 is brought into contact with the entire recess partition surface 12 (especially the partition bottom surface 12a).
  • the electroless plating solution 50 used here is the electroless ruthenium plating solution described above (see samples 1-9 in Tables 1-8).
  • electroless plating is performed while the recess 11 is kept filled with the electroless plating solution 50 and the electroless plating solution 50 is brought into contact with the recess partition surface 12 (especially the partition bottom surface 12a).
  • a plating body 40 containing ruthenium is deposited in the recess 11, and finally the entire recess 11 is filled with ruthenium as the plating body 40 (see FIG. 1C).
  • ruthenium (plating body 40) is selectively deposited on the compartment bottom face 12a without depositing ruthenium (plating body 40) on the compartment side face 12b at all or very little. takes the form of deposition. Therefore, according to the present example, ruthenium (plated body 40) can be embedded in the entire recess 11 while effectively avoiding any voids remaining in the recess 11 .
  • the ruthenium plated body 40 embedded in the recess 11 in this way can be used as wiring.
  • the element ratio of oxygen in the plating body 40 deposited in the recess 11 using the electroless ruthenium plating solution is 20% or less, and the element ratio of ruthenium is 80% or more.
  • the heat treatment of the plated body 40 in the recess 11 may be further performed using a forming gas composed of a mixed gas of nitrogen and hydrogen.
  • the element ratio of oxygen in the plating body 40 deposited in the recess 11 can be set to 10% or less, and the element ratio of ruthenium can be set to 90% or more. Ruthenium purity can be improved.
  • the substrate 10 can then undergo any processing to achieve the desired semiconductor substrate configuration.
  • FIGS. 2A to 2C are enlarged cross-sectional views of the substrate 10 showing an example of the second manufacturing method of the wiring substrate.
  • the same reference numerals are given to the same or corresponding elements as in the first manufacturing method shown in FIGS. will not be described in detail.
  • a substrate 10 having a seed layer 25 provided on an insulating film 20 is prepared.
  • the seed layer 25 promotes deposition of plating metal (ruthenium) in electroless plating, and the plating metal is deposited.
  • Seed layer 25 may have any composition that facilitates deposition of ruthenium as the plating metal.
  • a ruthenium thin film formed on the insulating film 20 by CVD can be used as the seed layer 25 .
  • a recess partition surface 12 (that is, a partition bottom surface 12 a and a partition side surface 12 b ) that partitions the recess portion 11 is formed of the seed layer 25 .
  • the recessed partition surface 12 of the present example includes seed layer 25 over its entirety, only a portion of recessed partition surface 12 may include seed layer 25 .
  • the electroless plating solution 50 is applied onto the substrate 10 to form a puddle of the electroless plating solution 50, and the recesses 11 are entirely filled with the electroless plating solution 50 as shown in FIG. 2B. This ensures that the electroless plating solution 50 is in contact with the recessed partition surface 12 (that is, the seed layer 25).
  • the electroless plating solution 50 used here is the electroless ruthenium plating solution described above (see samples 1-9 in Tables 1-8).
  • electroless plating is performed in a state in which the recess 11 is kept filled with the electroless plating solution 50 and the electroless plating solution 50 is brought into contact with the recess partition surface 12 (that is, the seed layer 25).
  • the recess partition surface 12 that is, the seed layer 25.
  • ruthenium is gradually deposited on the seed layer 25, and finally the ruthenium as the plating body 40 is embedded in the entire recess 11 (see FIG. 2C).
  • FIG. 3 is an enlarged cross-sectional view of the substrate 10 showing an example of the third manufacturing method of the wiring substrate.
  • the same reference numerals are given to the same or corresponding elements as in the first and second manufacturing methods described above, and the same items as in the first and second manufacturing methods will not be described in detail.
  • a barrier film 21 is provided on the insulating film 20 , and the recess partitioning surfaces 12 (that is, partition bottom surface 12 a and partition side surfaces 12 b ) that partition the recess 11 are formed by the barrier film 21 .
  • a substrate 10 is prepared.
  • Catalyst particles 29 adhere to the barrier film 21 (especially the surface range including the recessed partition surface 12).
  • the catalyst particles 29 are catalyst nuclei that promote deposition of plating metal (ruthenium) in electroless plating.
  • Catalyst particles 29 may have any composition (eg, palladium (Pd)) that promotes deposition of ruthenium as the plating metal.
  • a liquid (metal ion-containing liquid) in which metal ions that form the catalyst particles 29 are dispersed is applied onto the substrate 10 (barrier film 21), and the metal ion-containing liquid is applied to the barrier film using a rinsing liquid or the like.
  • Catalyst particles 29 can adhere to barrier film 21 by removing from above 21 .
  • the electroless plating solution is applied onto the substrate 10 to form a puddle of the electroless plating solution, and the recesses 11 are entirely filled with the electroless plating solution 50 .
  • electroless plating is performed in a state in which the recesses 11 are kept filled with the electroless plating solution, and the electroless plating solution is brought into contact with the recess partition surfaces 12 to which the catalyst particles 29 are attached.
  • deposition of ruthenium is promoted by the catalyst particles 29 , and finally the entire recess 11 is filled with ruthenium as the plated body 40 .
  • the above-described electroless ruthenium plating solution is brought into contact with the recess partition surface 12 that defines the wiring recesses 11 of the substrate 10, and the recesses 11 are formed by electroless plating.
  • a plating body 40 containing ruthenium may be deposited. Thereby, ruthenium can be stably deposited on the material by electroless plating.
  • the technical category that embodies the above technical idea is not limited.
  • the devices described above may be applied to other devices.
  • the above technical idea may be embodied by a computer program for causing a computer to execute one or more procedures (steps) included in the above method.
  • the above technical idea may be embodied by a computer-readable non-transitory recording medium in which such a computer program is recorded.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)

Abstract

Solution de dépôt autocatalytique comprenant un sel de ruthénium, un agent complexant, un agent réducteur et un régulateur de pH. L'agent réducteur comprend de l'hydrate d'hydrazine. L'agent complexant comprend de l'acide tartrique et du chlorure d'ammonium.
PCT/JP2022/046027 2021-12-24 2022-12-14 Solution de dépôt autocatalytique et procédé de fabrication de substrat de câblage WO2023120318A1 (fr)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000073176A (ja) * 1998-06-10 2000-03-07 Dow Corning Corp シリルハイドライド機能性樹脂上への非電解金属析出法
US20040084773A1 (en) * 2002-10-31 2004-05-06 Johnston Steven W. Forming a copper diffusion barrier
JP2004335459A (ja) * 2003-04-18 2004-11-25 Ube Ind Ltd 金属担持多孔質炭素膜、燃料電池用電極及びそれを用いた燃料電池
JP2005051185A (ja) * 2003-07-31 2005-02-24 Toshiba Corp 熱処理方法及び半導体装置の製造方法
JP2008112772A (ja) * 2006-10-30 2008-05-15 Toshiba Corp 半導体装置の製造方法
JP2008117853A (ja) * 2006-11-01 2008-05-22 Toshiba Corp 半導体装置およびその製造方法
US20080146042A1 (en) * 2000-05-15 2008-06-19 Asm International N.V. Method of growing electrical conductors
CN113106507A (zh) * 2021-04-15 2021-07-13 电子科技大学 一种用于微纳沟槽和盲孔填充的电镀钌镀液及配制方法
JP2021529435A (ja) * 2018-06-30 2021-10-28 ラム リサーチ コーポレーションＬａｍ Ｒｅｓｅａｒｃｈ Ｃｏｒｐｏｒａｔｉｏｎ ライナの不動態化および接着性改善のための金属ライナのジンケート処理およびドーピング

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000073176A (ja) * 1998-06-10 2000-03-07 Dow Corning Corp シリルハイドライド機能性樹脂上への非電解金属析出法
US20080146042A1 (en) * 2000-05-15 2008-06-19 Asm International N.V. Method of growing electrical conductors
US20040084773A1 (en) * 2002-10-31 2004-05-06 Johnston Steven W. Forming a copper diffusion barrier
JP2004335459A (ja) * 2003-04-18 2004-11-25 Ube Ind Ltd 金属担持多孔質炭素膜、燃料電池用電極及びそれを用いた燃料電池
JP2005051185A (ja) * 2003-07-31 2005-02-24 Toshiba Corp 熱処理方法及び半導体装置の製造方法
JP2008112772A (ja) * 2006-10-30 2008-05-15 Toshiba Corp 半導体装置の製造方法
JP2008117853A (ja) * 2006-11-01 2008-05-22 Toshiba Corp 半導体装置およびその製造方法
JP2021529435A (ja) * 2018-06-30 2021-10-28 ラム リサーチ コーポレーションＬａｍ Ｒｅｓｅａｒｃｈ Ｃｏｒｐｏｒａｔｉｏｎ ライナの不動態化および接着性改善のための金属ライナのジンケート処理およびドーピング
CN113106507A (zh) * 2021-04-15 2021-07-13 电子科技大学 一种用于微纳沟槽和盲孔填充的电镀钌镀液及配制方法

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